CN107447280A - A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use - Google Patents
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use Download PDFInfo
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- CN107447280A CN107447280A CN201710705134.7A CN201710705134A CN107447280A CN 107447280 A CN107447280 A CN 107447280A CN 201710705134 A CN201710705134 A CN 201710705134A CN 107447280 A CN107447280 A CN 107447280A
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- quantum dot
- graphene quantum
- polyvinyl alcohol
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/08—Addition of substances to the spinning solution or to the melt for forming hollow filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, belongs to electrostatic spinning field.The invention provides a kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, graphene quantum dot is well mixed by the present invention according to a certain percentage in a solvent with polyvinyl alcohol is made shell solution, using oily substance as sandwich layer solution, by coaxial electrostatic spinning, wash and be dried to obtain that specific surface area is big, flexible strong and with fluorescent effect graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use.Present invention process flow is simple, easy to operate, green non-pollution, and cost is low and is easy to industrialized production.Resulting hollow structure nanofiber has huge application prospect in photoelectric device, pharmaceutical carrier, flexible electronic device and anti-counterfeiting mark etc..
Description
Technical field
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, belongs to electrostatic spinning field.
Background technology
Electrostatic spinning technique is to carry out spinning under normal temperature, high pressure using polymer solution so as to obtain micron, sub-micron
With a kind of method of fiber in nanometer range.Nanofiber homogeneity made from electrostatic spinning technique is high, and its web has hole
The many advantages such as gap rate is high, the big, good permeability of specific surface area, lead in biomaterial for medical purpose, ionic adsorption, wastewater treatment etc.
Domain is applied widely.Coaxial electrostatic spinning is a kind of common technology for preparing core shell structure fiber.Coaxial electrostatic spinning
Method has less limitation to polymer, is usually used in preparing different types of core-shell type nanofiber, and in biomedical, medicine
The fields such as sustained release, biodegradation material possess very big application prospect.Polyvinyl alcohol is to be hydrolyzed to make by polyvinyl acetate resins
The white powder obtained, referred to as PVA.Polyvinyl alcohol is a kind of water miscible material, has good biocompatibility, biology can
Degradability, and film forming and better mechanical property, it is one of conventional electrostatic spinning polymer.
Graphene quantum dot is the carbon nanomaterial of quasi-zero dimension, has excellent dissolubility and chemical inertness, stable glimmering
Optical property and hypotoxicity, small to environmental hazard of preparation cost are cheap.Graphene quantum dot biological image, pharmaceutical carrier,
The fields such as OLED is shown, solar cell, biology sensor have broad application prospects.
Graphene quantum dot can prepare composite nano-fiber membrane with polyvinyl alcohol cospinning in existing preparation method.Than
Such as a kind of A of patent CN 104963022 " preparation methods of the graphene quantum dot composite fibre of high strength and modulus polyvinyl alcohol one
And product " in configured the mixed liquor of graphene quantum dot and polyvinyl alcohol water after, filtered and deaeration handles to obtain PVA-GQD
Spinning solution, by wet spinning, saturated aqueous sodium sulfate coagulating bath handles to obtain PVA-GQD as-spun fibres, to nascent fibre
Tie up multistage hot-stretch and thermal finalization and obtain high strength and modulus PVA-GQD composite fibres.This method solves to a certain extent
The strength problem of PVA fibers, but the technique spinning line is complicated, cost is high.The invention is using traditional spinning skill
Art is compound with polyvinyl alcohol by graphene quantum dot, it is therefore intended that the mechanical strength of vinal is improved, because gained produces
Thing does not have hollow structure, can not ensure that graphene quantum dot is distributed in the surface of fiber, therefore products therefrom does not have fluorescence
Effect.
Graphene quantum dot is dispersed in polyvinyl alcohol hollow Nano fiber in use by the present invention using coaxial electrostatic spinning technology
Outer surface, the hollow Nano fiber in use composite wood of graphene quantum dot and polyvinyl alcohol is obtained through removing sandwich layer solution and drying process
Material, products therefrom have the advantages that specific surface area big, flexible strong, fluorescent effect and biocompatibility.The letter of present invention process flow
Single, easy to operate, green non-pollution, cost is low and is easy to industrialized production, and products therefrom is in photoelectric device, pharmaceutical carrier, soft
Property electronic device and anti-counterfeiting mark etc. have huge application prospect.
The content of the invention
It is an object of the invention to solve the deficiencies in the prior art and shortcoming, there is provided a kind of flexibility is strong and has fluorescent effect
Hollow Nano fiber in use preparation method.This method is easy to operate, and production cost is low, is easy to large-scale production.The present invention is with poly-
Vinyl alcohol and the graphene oxide quantum dot of high dispersive through coaxial electrostatic spinning, removal sandwich layer solution and are done as shell material
Dry graphene quantum dot/polyvinyl alcohol the hollow Nano fiber in use for obtaining that there is hollow structure.This inventive method has that cost is low, work
The advantages that skill is simple, green, resulting hollow structure nanofiber is in photoelectric device, pharmaceutical carrier, flexible electronic device
Part and anti-counterfeiting mark etc. have huge application prospect.
The invention reside in provide a kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, its feature
It is:
(1) preparation of graphene quantum dot/polyvinyl alcohol spinning solution
Graphene quantum dot is dispersed in certain density poly-vinyl alcohol solution A, is uniformly dispersed to obtain graphene quantum
Point/polyvinyl alcohol shell spinning solution B;
(2) coaxial electrostatic spinning
Shell solution B and sandwich layer solution connect the outer layer and sandwich layer of coaxial electrostatic spinning syringe needle respectively, and adjustment syringe needle is away from connecing
Device to certain distance, connection HV generator is received to carry out coaxial electrostatic spinning, receive on the receiver with nucleocapsid knot
Graphene quantum dot/polyvinyl alcohol nano of structure;
(3) sandwich layer solution is removed
Graphene quantum dot/polyvinyl alcohol nano obtained by (2) step is put and washed in a solvent, until removing completely
Remove sandwich layer solution;
(4) drying process
(3) step products therefrom is dried and can obtain graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use.
The present invention is after adopting the above technical scheme, mainly have the following effects:
The methods of 1 the inventive method is using mechanical agitation, ultrasonic disperse, coaxial electrostatic spinning, technique is simple, operation side
Just, it is advantageously implemented large-scale production;
2 the inventive method are production process energy consumption is low, production security is good, green, production cost is low, and this hair
Bright method can be widely used for preparing graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use;
The graphene quantum dot that 3 present invention prepare/polyvinyl alcohol hollow Nano fiber in use uses less graphene quantum
The features such as point, products therefrom has fluorescent effect, flexible strong, and specific surface area is big, and have good biocompatibility, biology can
Degradability and nontoxicity.
Embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
The preparation method of a kind of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, it is characterised in that methods described
Comprise the following steps that:
(1) preparation of graphene quantum dot/polyvinyl alcohol spinning solution
Graphene quantum dot is dispersed in 50mg/ml polyvinyl alcohol water solution A, 24h is stirred at 60 DEG C and is uniformly dispersed
Obtain coaxial spinning shell solution B, the concentration of graphene quantum dot is 0.5mg/ml in B;
(2) preparation of graphene quantum dot/polyvinyl alcohol nano
Shell solution B and sandwich layer solution mineral oil connect the shell and sandwich layer of coaxial electrostatic spinning syringe needle respectively, adjust pin
Head distance receives roller 10cm, shell fltting speed 0.01ml/min, sandwich layer fltting speed 0.005ml/min, and connection high pressure is quiet
Electric generator carries out coaxial electrostatic spinning using 10KV high pressures, and the graphene amount with core shell structure is received on roller is received
Sub- point/polyvinyl alcohol nano;
(3) sandwich layer solution is removed
Graphene quantum dot/polyvinyl alcohol nano obtained by (2) step is placed in normal octane and washs 24h, completely
Remove sandwich layer mineral oil;
(4) drying process
(3) step products therefrom is placed in 80 DEG C of air dry ovens be dried 12h can obtain graphene quantum dot/
Polyvinyl alcohol hollow Nano fiber in use.
Embodiment 2
The preparation method of a kind of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, it is characterised in that methods described
Comprise the following steps that:
(1) preparation of graphene quantum dot/polyvinyl alcohol spinning solution
Graphene quantum dot is dispersed in 120mg/ml polyvinyl alcohol water solution A, 24h is stirred at 80 DEG C and is uniformly dispersed
Obtain coaxial spinning shell solution B, the concentration of graphene quantum dot is 10mg/ml in B;
(2) preparation of graphene quantum dot/polyvinyl alcohol nano
Shell solution B and sandwich layer solution mineral oil connect the shell and sandwich layer of coaxial electrostatic spinning syringe needle respectively, adjust pin
Head distance receives roller 15cm, shell fltting speed 0.02ml/min, sandwich layer fltting speed 0.01ml/min, connects high-pressure electrostatic
Generator carries out coaxial electrostatic spinning using 15KV high pressures, and the graphene quantum with core shell structure is received on roller is received
Point/polyvinyl alcohol nano;
(3) sandwich layer solution is removed
Graphene quantum dot/polyvinyl alcohol nano obtained by (2) step is placed in normal octane and washs 48h, completely
Remove sandwich layer mineral oil;
(4) drying process
(3) step products therefrom is placed in 80 DEG C of air dry ovens be dried 24h can obtain graphene quantum dot/
Polyvinyl alcohol hollow Nano fiber in use.
Embodiment 3
The preparation method of a kind of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, it is characterised in that methods described
Comprise the following steps that:
(1) preparation of graphene quantum dot/polyvinyl alcohol spinning solution
Graphene quantum dot is dispersed in 150mg/ml polyvinyl alcohol water solution A, 24h is stirred at 90 DEG C and is uniformly dispersed
Obtain coaxial spinning shell solution B, the concentration of graphene quantum dot is 15mg/ml in B;
(2) preparation of graphene quantum dot/polyvinyl alcohol nano
Shell solution B and sandwich layer solution mineral oil connect the shell and sandwich layer of coaxial electrostatic spinning syringe needle respectively, adjust pin
Head distance receives roller 20cm, shell fltting speed 0.02ml/min, sandwich layer fltting speed 0.005ml/min, and connection high pressure is quiet
Electric generator carries out coaxial electrostatic spinning using 20KV high pressures, and the graphene amount with core shell structure is received on roller is received
Sub- point/polyvinyl alcohol nano;
(3) sandwich layer solution is removed
Graphene quantum dot/polyvinyl alcohol nano obtained by (2) step is placed in normal octane and washs 48h, completely
Remove sandwich layer mineral oil;
(4) drying process
(3) step products therefrom is placed on and 48h is dried in 100 DEG C of air dry ovens can obtain graphene quantum
Point/polyvinyl alcohol hollow Nano fiber in use.
Embodiment 4
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (1) step, the volume ratio of absolute ethyl alcohol and deionized water is 1 in the solution A:9ml/ml, graphite in B solution
The concentration of alkene quantum dot is 8mg/ml;
In (2) step, the sandwich layer solution is dimethicone;
In (3) step, the detergent is acetone.
Embodiment 5
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (1) step, the volume ratio of absolute ethyl alcohol and deionized water is 2 in the solution A:8ml/ml, graphite in B solution
The concentration of alkene quantum dot is 8mg/ml;
In (2) step, the sandwich layer solution is methyl-silicone oil, and reception device receives for flat board copper foil;
In (3) step, the detergent is n-hexane.
Embodiment 6
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (1) step, the volume ratio of absolute ethyl alcohol and deionized water is 3 in the solution A:7ml/ml, graphite in B solution
The concentration of alkene quantum dot is 10mg/ml;
In (2) step, the sandwich layer solution is methyl-silicone oil, and reception device receives for flat board copper foil;
In (3) step, the detergent is hexamethylene.
Embodiment 7
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (1) step, the volume ratio of absolute ethyl alcohol and deionized water is 4 in the solution A:6ml/ml, graphite in B solution
The concentration of alkene quantum dot is 10mg/ml;
In (2) step, the sandwich layer solution is edible oil, and reception device receives for flat board aluminium foil;
In (3) step, the detergent is normal octane.
Embodiment 8
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (1) step, the volume ratio of absolute ethyl alcohol and deionized water is 5 in the solution A:5ml/ml, by graphene amount
Son point is dispersed in poly-vinyl alcohol solution A, and 24h is stirred at 80 DEG C and is uniformly dispersed to obtain coaxial spinning shell solution B, in B solution
The concentration of graphene quantum dot is 10mg/ml.
Embodiment 9
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (2) step, the sandwich layer solution is methyl-silicone oil, and reception device receives for flat board aluminium foil;
In (3) step, the detergent is normal heptane.
Embodiment 10
A kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, with embodiment 1, wherein:
In (2) step, the sandwich layer solution is methyl-silicone oil, and reception device receives for flat board copper foil;
In (3) step, the detergent is hexamethylene and acetone, volume ratio 9:1ml/ml.
Claims (2)
- A kind of 1. preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use, it is characterised in that:(1) preparation of graphene quantum dot/polyvinyl alcohol spinning solutionGraphene quantum dot is dispersed in certain density poly-vinyl alcohol solution A, is uniformly dispersed to obtain graphene quantum dot/poly- Vinyl alcohol shell spinning solution B;(2) coaxial electrostatic spinningShell solution B and sandwich layer solution connect the outer layer and sandwich layer of coaxial electrostatic spinning syringe needle respectively, and adjustment syringe needle is away from receiver To certain distance, connection HV generator carries out coaxial electrostatic spinning, receives on the receiver with core shell structure Graphene quantum dot/polyvinyl alcohol nano;(3) sandwich layer solution is removedGraphene quantum dot/polyvinyl alcohol nano obtained by (2) step is put and washed in a solvent, until removing coring completely Layer solution;(4) drying process(3) step products therefrom is dried and can obtain graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use.
- 2. a kind of preparation method of graphene quantum dot/polyvinyl alcohol hollow Nano fiber in use according to claim 1, it is special Sign is:2.1) for the diameter of graphene quantum dot described in step (1) in 1~20nm, the number of plies is 1~5 layer;2.2) concentration of step (1) polyvinyl alcohol spinning solution is 50~160mg/ml, in poly-vinyl alcohol solution A, anhydrous second The volume ratio of alcohol and deionized water is 1:9~3:2ml/ml;2.3) in graphene quantum dot described in step (1)/polyvinyl alcohol shell spinning solution B, the concentration of graphene quantum dot For 0.5~15mg/ml;2.4) sandwich layer solution used in step (2) be oily substance, can for mineral oil or methyl-silicone oil or dimethicone or One or more in edible oil, the kinematic viscosity of sandwich layer material is 12~1000mm2/s;2.5) coaxial electrostatic spinning parameter is in step (2):Coaxial syringe needle sandwich layer internal diameter used is 0.1~1mm, in shell syringe needle Footpath is 0.8~10mm, and syringe needle is 0.008~0.02ml/min apart from 10~25cm of reception device, shell flow velocity, and sandwich layer flow velocity is 0.002~0.005ml/min, coaxial electrostatic spinning is carried out using 10~25KV high pressure ranges;2.6) receiver can be that roller receives or flat board receives in step (2), and it is copper foil or aluminium foil to receive material;2.7) solvent that sandwich layer solution is removed in step (3) can be acetone or normal octane or n-hexane or hexamethylene or normal heptane It is one or two kinds of;2.8) drying temperature is 60~100 DEG C in step (4), and drying time is 4~48 hours.
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Cited By (7)
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CN108159493A (en) * | 2017-12-28 | 2018-06-15 | 山东省日照市人民医院 | A kind of preparation method of alginate-hydrogel nano fiber scaffold |
CN109929539A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | Flexible luminescent material and preparation method thereof |
CN110060874A (en) * | 2019-04-25 | 2019-07-26 | 上海交通大学 | The preparation method of flexible super capacitor electrode |
CN110773005A (en) * | 2019-11-07 | 2020-02-11 | 中国计量大学 | Device for treating wastewater based on graphene oxide quantum dot modified polysulfone ultrafiltration membrane |
CN112030269A (en) * | 2020-09-04 | 2020-12-04 | 安徽瑜合警用装备有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
CN114507915A (en) * | 2022-01-25 | 2022-05-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fluorescent composite fiber and preparation method and application thereof |
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CN109929539B (en) * | 2017-12-15 | 2020-07-21 | Tcl科技集团股份有限公司 | Flexible luminescent material and preparation method thereof |
CN108159493A (en) * | 2017-12-28 | 2018-06-15 | 山东省日照市人民医院 | A kind of preparation method of alginate-hydrogel nano fiber scaffold |
CN108159493B (en) * | 2017-12-28 | 2020-11-20 | 山东省日照市人民医院 | Preparation method of alginate-hydrogel nanofiber scaffold |
CN110060874A (en) * | 2019-04-25 | 2019-07-26 | 上海交通大学 | The preparation method of flexible super capacitor electrode |
CN110773005A (en) * | 2019-11-07 | 2020-02-11 | 中国计量大学 | Device for treating wastewater based on graphene oxide quantum dot modified polysulfone ultrafiltration membrane |
CN110773005B (en) * | 2019-11-07 | 2021-09-24 | 中国计量大学 | Device for treating wastewater based on graphene oxide quantum dot modified polysulfone ultrafiltration membrane |
CN112030269A (en) * | 2020-09-04 | 2020-12-04 | 安徽瑜合警用装备有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
CN112030269B (en) * | 2020-09-04 | 2023-02-03 | 安徽德和织造有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
CN114507915A (en) * | 2022-01-25 | 2022-05-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fluorescent composite fiber and preparation method and application thereof |
CN114507915B (en) * | 2022-01-25 | 2024-03-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fluorescent composite fiber and preparation method and application thereof |
CN115624869A (en) * | 2022-07-26 | 2023-01-20 | 青岛大学 | Graphene quantum dot antibacterial adsorption electrostatic spinning nanofiltration membrane and preparation method thereof |
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Application publication date: 20171208 |